Abstract: In order to enable students to deeply understand the academic frontier of hot research fields such as photocatalysis and master the preparation methods of low dimensional nanocomposites, an undergraduate comprehensive experiment of the effect of fabrication of 1D/2D inorganic/organic heterostructure on the visible-light-driven photocatalytic water splitting performance to produce hydrogen is designed. 1D nanorod and 2D nanosheet heterostructure was fabricated via a facile mixing-calcination method, and the intimate interface of heterostructure remarkably promotes the charge separation of photogenerated carriers, greatly improving the hydrogen production rate of photocatalytic water splitting. The experiment design possesses strong comprehensiveness and close combination between basic knowledge and experimental result, which is conducive to stimulate students’ innovative thinking and cultivate students’ comprehensive literacy.